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Kavalactones Extraction

Bwiggy

I like plants
Hi @winpg. How is your extraction process going?
I would like to learn from your experience if you are willing to share.
 

Groggy

Kava aficionado
Admin
Hi @winpg. How is your extraction process going?
I would like to learn from your experience if you are willing to share.
Absolutely, as soon as I have results, I will certainly share, frankly I am still undecided on the extraction method, there are mixed feeling on the extraction method using ethanol, so I am looking into other possibilities as of now.
 

verticity

I'm interested in things
Fair enough. Thanks.
Is this the machine that was mentioned earlier?
http://www.ebay.com/itm/Millipore-W...796731?hash=item360200207b:g:DogAAOSwwIZXTJ2z
That's an HPLC pump, which is just part of a complete HPLC system. You also need a column and a detector... The current bid is $39?? That's hard to believe...there must be something wrong with it... Oh, I see, you can't buy it for that price; you have to make a bid.. It will certainly sell for more than that. e.g.
http://www.ebay.com/itm/Waters-510-...illipore-115-230v-50-60hz-250-VA/162025749724
$250
So you might be able to put together a complete HPLC from used parts like this for a couple thousand $ or so.
 

Groggy

Kava aficionado
Admin
That's an HPLC pump, which is just part of a complete HPLC system. You also need a column and a detector... The current bid is $39?? That's hard to believe...there must be something wrong with it... Oh, I see, you can't buy it for that price; you have to make a bid.. It will certainly sell for more than that. e.g.
http://www.ebay.com/itm/Waters-510-...illipore-115-230v-50-60hz-250-VA/162025749724
$250
So you might be able to put together a complete HPLC from used parts like this for a couple thousand $ or so.
What I was thinking other than ethanol is the CO2 extraction, but I have to look into costs on that, I know it's considerably more, but the kava community seems to accept unanimously as the best and most efficient way to extract.
Also if this becomes something I want to sell, I want to have the support of the community and not be singled out for using ethanol.
 

verticity

I'm interested in things
What I was thinking other than ethanol is the CO2 extraction, but I have to look into costs on that, I know it's considerably more, but the kava community seems to accept unanimously as the best and most efficient way to extract.
Also if this becomes something I want to sell, I want to have the support of the community and not be singled out for using ethanol.
The only thing is that no one has proved to my satisfaction that CO2 actually is safer. It is definitely trendy, though. Here is a "cheap" supercritical CO2 extractor ($3200):
http://ocolabs.com/extractors/
You may be able to get a used one for less..
 

Groggy

Kava aficionado
Admin
The only thing is that no one has proved to my satisfaction that CO2 actually is safer. It is definitely trendy, though. Here is a "cheap" supercritical CO2 extractor ($3200):
http://ocolabs.com/extractors/
You may be able to get a used one for less..
I didn't realize it was that expensive, I will have to rethink this. From my 6+ years experience in vaping I know of some flavors being extracted via ethanol. and as I believe @Ligermeat was saying, ethanol extraction gets a bad rap when it shouldn't. I will do more research on it before moving forward one way or another.
A third option is cold press extraction, but this option is not necessarily cheaper, ranging fromm $400-$4K, by the looks of it, this machine is in the higher price range.
 
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Palmetto

Thank God!
I think some of the suggestions here are too complicated for home users. I worked several years in biophysics and chemistry labs, learning a few tricks along the way. Some paper I read recently tested several solvents for kavalactone (KL) extraction efficiency, and found that ethanol was most efficient. Because KLs are technically semipolar, they have better affinity for alcohols and amphipathic surfactants, like lecithin. Ethanol can travel across cell membranes, as well as assist solutes in crossing membranes. With a medium grind, you probably have a good bit of the KLs stuck inside of the cells that might not escape well with water extraction. Sonication would also help with the membrane release issue.

Back to the paper I read, it showed very high extraction rates for KLs with ethanol, and less extraction with acetone and pure hydrocarbons. This is a good thing, because it suggests that the ideal dielectric constant for solution of KLs is not extremely polar, thus you can probably have a bit of water mixed with the ethanol and still get pretty good results. Recently, I have been soaking medium grind with in a small volume of solution that is 20% ethanol + 10% lecithin + 70% water overnight as a thick paste. This allows for the KLs to slowly permeate the membranes, and hopefully partition into the lecithin. My goal is to make the solvent mixture to be at least as attractive to the KLs as the powder itself, so when I strain it and dilute it, the KLs don't jump right back to the powder. Sometimes I blend it, sometimes I don't.

What I find is that the taste becomes more bitter, and somewhat more nauseating, but still tolerable. I suspect that this is because I am extracting a greater percentage of DHM/DHK than before, but I don't have proof of this. I can say that it makes a much much stronger and more body heavy drink than by using water extraction.
 

Bwiggy

I like plants
HI @Palmetto - I appreciate your comments. Would you willing to post a video of your method?
I'd like to see it... and really get what happens to the ethanol.
Also, I have one of those jewelry cleaners that cleans by signification. I bought it specifically for kava. It's big. Like it could hold a half a gallon of liquid probably. Do you know how long signification is needed - or at what point it stops being effective?
Edit:my autocorrect kept making "sonification" into "signification"
 
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Groggy

Kava aficionado
Admin
I think some of the suggestions here are too complicated for home users. I worked several years in biophysics and chemistry labs, learning a few tricks along the way. Some paper I read recently tested several solvents for kavalactone (KL) extraction efficiency, and found that ethanol was most efficient. Because KLs are technically semipolar, they have better affinity for alcohols and amphipathic surfactants, like lecithin. Ethanol can travel across cell membranes, as well as assist solutes in crossing membranes. With a medium grind, you probably have a good bit of the KLs stuck inside of the cells that might not escape well with water extraction. Sonication would also help with the membrane release issue.

Back to the paper I read, it showed very high extraction rates for KLs with ethanol, and less extraction with acetone and pure hydrocarbons. This is a good thing, because it suggests that the ideal dielectric constant for solution of KLs is not extremely polar, thus you can probably have a bit of water mixed with the ethanol and still get pretty good results. Recently, I have been soaking medium grind with in a small volume of solution that is 20% ethanol + 10% lecithin + 70% water overnight as a thick paste. This allows for the KLs to slowly permeate the membranes, and hopefully partition into the lecithin. My goal is to make the solvent mixture to be at least as attractive to the KLs as the powder itself, so when I strain it and dilute it, the KLs don't jump right back to the powder. Sometimes I blend it, sometimes I don't.

What I find is that the taste becomes more bitter, and somewhat more nauseating, but still tolerable. I suspect that this is because I am extracting a greater percentage of DHM/DHK than before, but I don't have proof of this. I can say that it makes a much much stronger and more body heavy drink than by using water extraction.
Does adding the 20% ethanol affect the end product, in other words, are you drinking kava with 20% alcohol content or does that evaporate in the overnight process?
 

Palmetto

Thank God!
I think you mean a "sonicator". Years ago, I worked in a number of labs with various sonicators. The cheap jeweler bath style for about $4000, or the higher powered probe style.

After I soak root powder in an aqueous ethanol/lecithin solution, I add some hot water, squeeze out the liquid a few times, then usually add more room temperature water and/or citrusy flavored coke to improve the taste. The ethanol/lecithin solution is intended to extract the kavalactones out of the root. Once I remove the root, then the kavalactones can't partition back into it, but can adsorb onto the surface of the container/mug I have it in. Some people don't do a second wash, but occasionally I do a fourth wash, because I can still extract kavalactones out to a lesser extent, then I use fresh root to strengthen the weak grog. I am gradually lessening the ethanol content I am using. Like I mentioned previously, there is logically a sweet spot where more kavain is extracted, but the flavokawain (flavokavain) B levels are still minimal.

As I also mentioned before, I have the feeling that the grog is less heady with the ethanol/lecithin solution than with pure water. I'm still trying to figure out what I like best. I've gone through only 7-8 lbs. of powder so far, so I am still learning.
 

verticity

I'm interested in things
I think some of the suggestions here are too complicated for home users. I worked several years in biophysics and chemistry labs, learning a few tricks along the way. Some paper I read recently tested several solvents for kavalactone (KL) extraction efficiency, and found that ethanol was most efficient. Because KLs are technically semipolar, they have better affinity for alcohols and amphipathic surfactants, like lecithin. Ethanol can travel across cell membranes, as well as assist solutes in crossing membranes. With a medium grind, you probably have a good bit of the KLs stuck inside of the cells that might not escape well with water extraction. Sonication would also help with the membrane release issue.

Back to the paper I read, it showed very high extraction rates for KLs with ethanol, and less extraction with acetone and pure hydrocarbons. This is a good thing, because it suggests that the ideal dielectric constant for solution of KLs is not extremely polar, thus you can probably have a bit of water mixed with the ethanol and still get pretty good results. Recently, I have been soaking medium grind with in a small volume of solution that is 20% ethanol + 10% lecithin + 70% water overnight as a thick paste. This allows for the KLs to slowly permeate the membranes, and hopefully partition into the lecithin. My goal is to make the solvent mixture to be at least as attractive to the KLs as the powder itself, so when I strain it and dilute it, the KLs don't jump right back to the powder. Sometimes I blend it, sometimes I don't.

What I find is that the taste becomes more bitter, and somewhat more nauseating, but still tolerable. I suspect that this is because I am extracting a greater percentage of DHM/DHK than before, but I don't have proof of this. I can say that it makes a much much stronger and more body heavy drink than by using water extraction.
Yup, KLs are semi-polar, not non-polar. They are highly soluble in ethanol (semi-polar), and poorly soluble in water (polar) and hexane (non-polar). The interesting thing is that I looked at the partition coeffecients of KLs vs. flavokavains a while ago, and the flavokavains are actually significantly less polar than the KLs. In other words, they ought to be more soluble in hexane and less so in ethanol than KLs. So.. it is possible that ethanol extraction could actually deplete FKs. It is also possible that CO2 could enhance FKs because of similar considerations. That is why I am a CO2 skeptic.
 

verticity

I'm interested in things
...
After I soak root powder in an aqueous ethanol/lecithin solution, I add some hot water, squeeze out the liquid a few times, then usually add more room temperature water and/or citrusy flavored coke to improve the taste. ...
If the citrusy flavored soda you are adding contains ascorbic acid that could account for the increased body effect. Ascorbic acid is a reducing agent which can react with the double bond of kavain to change it into DHK. You can avoid this by using something that contains only citric acid, but not ascorbic acid.
 

Palmetto

Thank God!
Perhaps I can accentuate the reducing effect as well and compare against the non ascorbic mixture. Do you have a reference for the measure of polarity you mentioned? I tend to use dielectric constants, but others prefer other indices. I had some great success solving challenges in the lab by fine tuning the overall dielectric constant of mixtures as a whole.
 

verticity

I'm interested in things
Perhaps I can accentuate the reducing effect as well and compare against the non ascorbic mixture. Do you have a reference for the measure of polarity you mentioned? I tend to use dielectric constants, but others prefer other indices. I had some great success solving challenges in the lab by fine tuning the overall dielectric constant of mixtures as a whole.
I used this site to calculate the partition coefficents of KLs and FKs.
For example, Kavain:
http://www.chemicalize.org/structure/#!mol=kavain&source=fp
has logP = 2.43
whereas FKB:
http://www.chemicalize.org/structure/#!mol=flavokavain+B&source=fp
has logP = 3.92
where logP is defined as:
"The partition coefficient is a ratio of concentrations of an un-ionized compound in the two phases of immiscible solvents (water and n-octanol) at equilibrium. logP is the 10-base logarithmic measure of the coefficient."
The calculation takes into account the polarity, polarizability (I think), and number of hydrogen bonding sites of the molecule.
 

Palmetto

Thank God!
If ascorbic acid modification works, then theoretically, you miht only need two different varieities of heady kava strains, and you could somewhat create a range of balanced or body heavy, yet noble kavas from that.
 

Groggy

Kava aficionado
Admin
I think you mean a "sonicator". Years ago, I worked in a number of labs with various sonicators. The cheap jeweler bath style for about $4000, or the higher powered probe style.

After I soak root powder in an aqueous ethanol/lecithin solution, I add some hot water, squeeze out the liquid a few times, then usually add more room temperature water and/or citrusy flavored coke to improve the taste. The ethanol/lecithin solution is intended to extract the kavalactones out of the root. Once I remove the root, then the kavalactones can't partition back into it, but can adsorb onto the surface of the container/mug I have it in. Some people don't do a second wash, but occasionally I do a fourth wash, because I can still extract kavalactones out to a lesser extent, then I use fresh root to strengthen the weak grog. I am gradually lessening the ethanol content I am using. Like I mentioned previously, there is logically a sweet spot where more kavain is extracted, but the flavokawain (flavokavain) B levels are still minimal.

As I also mentioned before, I have the feeling that the grog is less heady with the ethanol/lecithin solution than with pure water. I'm still trying to figure out what I like best. I've gone through only 7-8 lbs. of powder so far, so I am still learning.
The end result you are describing may fits my needs perfectly, I want an extract that's very strong for use as a vape base. That's why I started the thread, I wanted to know the most effective way to extract as many KL's as possible from a given amount of root. What would you tweak from the above for that purpose?
 
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